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Method for purifying electronic grade octamethylcyclotetrasiloxane

A technology of octamethylcyclotetrasiloxane and hexamethylcyclotetrasiloxane, which is applied in the field of purification of electronic-grade octamethylcyclotetrasiloxane, can solve the problems of eliminating uncleanness, and achieve a simple and convenient method Effect

Active Publication Date: 2014-05-14
SHANGHAI AIMO JINSHAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The conventional method is to rectify with a rectification device wrapped in quartz or polytetrafluoroethylene. However, due to the sublimation and volatility of trace heavy metals, the heavy metals that exist in the raw materials themselves will still sublimate and volatilize with the evaporation of the raw materials, thereby eliminating unnecessary clean

Method used

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  • Method for purifying electronic grade octamethylcyclotetrasiloxane
  • Method for purifying electronic grade octamethylcyclotetrasiloxane

Examples

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Effect test

Embodiment 1

[0018] 1 ton of octamethylcyclotetrasiloxane with a content of 99% (weight) enters the light removal tower of the electronic grade silane refining system through a silane compressor. The number of theoretical plates is 50. 0.03Mpa, the temperature at the bottom of the tower is heated by a temperature program until the temperature of the fraction received at the top of the tower is 96°C, which is mainly isolated hexamethylcyclotrisiloxane (D3) after detection. When the distillate volume becomes smaller and smaller until it does not come out, the temperature at the top of the tower begins to rise, and there is no D3 in the bottom component inspection.

[0019] The octamethylcyclotetrasiloxane that has been removed from D3 flows from the bottom of the tower into the reaction kettle of the de-heavy rectification tower, and the de-light tower restarts the next batch of rectification. Add 0.5kg of the high-efficiency ligand shown above to the reactor, heat to 100°C, react for 5 hour...

Embodiment 2

[0023] The octamethylcyclotetrasiloxane with a content of 99% (weight) enters the light removal tower of the electronic grade silane refining system through the silane compressor. The number of theoretical plates is 50. The light removal tower is operated under reduced pressure, and the pressure is maintained at 0.03Mpa , the temperature at the bottom of the tower was heated by a temperature program until the temperature of the fraction received at the top of the tower was 96°C. It was detected that it was mainly separated hexamethylcyclotrisiloxane (D3). When the distillate volume becomes smaller and smaller until it does not come out, the temperature at the top of the tower begins to rise, and there is no D3 in the bottom component inspection.

[0024] The octamethylcyclotetrasiloxane that has been removed from D3 flows from the bottom of the tower into the reaction kettle of the de-heavy rectification tower, and the de-light tower restarts the next batch of rectification. A...

Embodiment 3

[0028] The octamethylcyclotetrasiloxane with a content of 99% (weight) enters the light removal tower of the electronic grade silane refining system through the silane compressor. The number of theoretical plates is 50. The light removal tower is operated under reduced pressure, and the pressure is maintained at 0.03Mpa , the temperature at the bottom of the tower was heated by a temperature program until the temperature of the fraction received at the top of the tower was 96°C. It was detected that it was mainly separated hexamethylcyclotrisiloxane (D3). When the distillate volume becomes smaller and smaller until it does not come out, the temperature at the top of the tower begins to rise, and there is no D3 in the bottom component inspection.

[0029] The octamethylcyclotetrasiloxane that has been removed from D3 flows from the bottom of the tower into the reaction kettle of the de-heavy rectification tower, and the de-light tower restarts the next batch of rectification. T...

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Abstract

The invention relates to a method for purifying electronic grade octamethylcyclotetrasiloxane in a rectifying manner. The method comprises the following steps: (1) adding 99% of the octamethylcyclotetrasiloxane into a rectifying tower, and removing little residual hexamethylcyclotrisiloxane (D3 for short) from the top of the tower at 90-96 DEG C under the pressure of 0.02-0.03MPa; (2) enabling the octamethylcyclotetrasiloxane without the D3 to flow out of the tower and enter a reaction kettle of a de-heavy rectifying tower, adding 0.01%-0.1% by weight of a special efficient metal complex ligand, heating to 90-100 DEG C, reacting for 1-10 hours, and performing reduced pressure distillation. The de-heavy rectifying tower is arranged in a superclean room, the reduced pressure operation is adopted in the tower, the pressure of the tower is 0.005-0.01Mpa, the temperature of the top of the tower is 100-110 DEG C, more than 99.99% by weight of the octamethylcyclotetrasiloxane is received, and residues at the bottom of the tower are high-boiling-point impurities; the reaction kettle and the inner wall of the de-heavy rectifying tower and a pipeline receiving container are all wrapped with polytetrafluoroethylene, and fillers of the de-heavy rectifying tower are wrapped with the polytetrafluoroethylene.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a method for purifying electronic-grade octamethylcyclotetrasiloxane. Background technique [0002] Octamethylcyclotetrasiloxane (D4 for short), colorless transparent or milky white liquid, flammable, no peculiar smell, is a hydrolyzate based on dimethyldichlorosilane as the main raw material, which is obtained through the hydrolysis synthesis process Individually defined compounds obtained through separation and rectification, or separation and rectification of the hydrolyzate after cleavage. The primary form of dimethylcyclosiloxane is mainly used for ring-opening polymerization to form silicone oil, silicone rubber and silicone resin with different degrees of polymerization. These polymers are further processed into products that are widely used in various fields such as construction, electronics, textiles, automobiles, personal care, fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 姜标张黎明陈君诸平陈旭敏
Owner SHANGHAI AIMO JINSHAN PHARM CO LTD
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